Textile sizing



TEXTILE SIZING Henri Glbello, Paris, France, assignor to Societe Nobel Francaise, Paris, Seine, France, a jointstock company oi France No Drawint- Application December a, 1937, se-

rial No. 178,827. In France March 13, 193':

10 Claims. (Cl. 260-32) l 7 mp4 again The customary way of sizing textile fibres and starting substance and produces the sizing in 5 cloths made of these fibres is to impregnate or amedium which contains a polymerizing agent, coat with solutions or suspensions composed of a Tol'isticizer, solvents and an emulsifier... The various soluble substances in water, such as gums, emulsion produced is of the oil-in-water type and mucilages, glu t the polymer is retained in suspension in the These types of sizings present certain inconwater partly by the emulsifier and partly by alvenient features and cannot be used in all cases cohols of low molecular weight which are soluble occurring in practice. For example, they are ferin water and dissolve both the nonomeric and mentable, and due to fermentation exude an expolymeric vinyl acetate. The plasticizers used tremely disagreeable odor. Furthermore, they must be water soluble. The low molecular weight are soluble in water, and their fixing is generally alcohols, above referred to, act as intermediate fairly difiicult and. frequently impossible. Besolvents between the water and the monomeric sides they are not adapted for furnishing uniform and polymeric vinyl acetates. The plasticizers surfaces, 1. e. glazing the tissues on which they are soluble in both alcohol and water. are applied. Of the emulgents available for use in the siz- The present invention consists in that it has me, the product manufactured in Germany by 0 been found that it is possible to manufacture the I. G. Farbenindustrie Aktiengesellschaft, and sizings which do not present the inconveniences sold under the trade name of Emulphur-O has enumerated above, by using as a base substance a proven preferable because of the high viscosities polyvinyl acetate in the form of an aqueous 0f the emulsions obtainable with it. The comemulsion. position of this emulgent is set out in Melliand An object of the present invention is to pro- Textilberichte"-1935, page 511 to be a condencide a sizing for textiles which does not injure sation product of polymerized ethylene oxide the textiles and which does not require any subwith lauric alcohol, that is, a lauric ether of polysequent fixing to make it waterproof. ethylene oxide having the formula:

; Another object is to provide a sizing which may m be readily fixed to make it permanent and unc12H25(OC2H")"oH changeable by water Emulsions of various polymerized acrylic de- Another object is t provide a sizing which rivatives are known, but the emulsions prepared softens at body temperature so that garments according to the Present t on ave the 01- 30 made from textiles sized therewith adapt themlowlng characteristics! selves readily to the shape of the wearers body. (a) They contain a relatively ge a ount of A further object is to provide sized textiles emulsifying agent omlllgentn fact, emulwhich become soft and pliable at body tempera-' Sions 0f the type which av n pr pared here tures and adapt, ghemsewes t t body of t tofore, contain as emulgent small quantities of w weal-en sulphonic derivatives, such as alcoyl naphtha- 40 Another object is to produce a sizing by the line, which produce emulsions With a high deg ee polymerization of vinyl acetate in an emulsifypolymerisation and y loW Viscosity. The ing medium so that the product is immediately emulgent contemplated for use according to the available as a liquid sizing. present invention, is the above-mentioned prod- A still further object consists in providing a t known o t e ade under the name of 45 process which may be carried out under ordinary D This product s ed i fairly pressure conditions to produce a water and bac- Strong ce ation which may be from 5% to t m resistant sizing emulsion 20% of the quantity of monomeric vinyl acetate to It has already been proposed to use vinyl chlobe emulsified.

, ride polymers and the products of conjoint poly- (b) They contain an alcohol sufficiently Solu- 5o,

" merization of vinyl chloride and vinyl acetate ble in water and with a low boilin p nt wh in emulsified or dispersed forms to provide a. acts as third solvent. Among the substances waterproof textile sizing. The chlorides and ch y be used a e listed e y o other halides, however, have the effect of releasethyl alcohol, n-propyl alcohol, isopropyl alcohol ing halogen acids which eventually weaken and and isobutyl alcohol.

destroy the fabrics to which their compositions (0) They contain a slowly volatile component are applied. Vinyl chloride is a gas and vinyl which serves as a plasticizer for the emulsified bromide a low boiling liquid so that polymerizapolyvinyl acetate. Among the substances which tion of these substances must be conducted in may be used those are given preference which are closed containers at advanced pressures. The relatively soluble in water and which possess a m The present invention relates to improvements in textile sizings and the process of preparing same, and also the sized textiles obtained therey.

polymers of these halides cannot be completely I freed of halogen acids and, in addition to this, are unstable and gradually release these acids.

The present invention uses ginyl acetate as its free alcoholic function. Among the substances mentioned, benzyl alcohol is mentioned specifically.

The emulsion is prepared by heating its various components to reflux for a sufficiently long period for polymerizing the monomeric vinyl acetate in the presence of a polymerisation catalyst and any desired additions, such as for example pigments and fillers. It is essential that during t e entire polymerisation process the emulsion be stirred vigorously and that this stirring be continued until the finished emulsion be completely cooled. The polymerisation catalyst may be destroyed once the emulsion is completed. The product thus obtained shows remarkable stability, is easily diluted with water and can then be used in sizing textiles.

The emulsion, which generally is fairly liquid, may be applied, for example, by means of a brush, or just by steeping. Very frequently the sizing with vinyl emulsion base must be applied on the face of the fabric. In this case it is preferable to thicken the emulsion by means of aqueous solutions of natural gums or resins and to apply the thickened emulsion by means of a. scraper or spreading knife using the customary processes.

While sizings prepared as above are insoluble in water they undergo swelling when wet. To prevent swelling it is often desirable to fix the sizing. This may be accomplished by appropriate treatments, as with a caustic alkali solution, with ammonia gas, with organic bases, etc. It must be noted that fixing also improves resistance to water to a considerable degree in the case of mixed sizings containing vinyl resin emulsion as well as natural gums or mucilages.

One of the advantages of sizings made in accordance with the invention is that they may be successfully applied in cases where the sizing must soften at a given temperature. By way of example we mention sizings for the reverse side of velvets and felts intended for use in the hat trade or other purposes.

Fabrics of this sort are finding use in the making of close fitting garments of various types. A product produced according to the present invention ordinarily has a softening point around body temperature. Fabrics sized with such a product are relatively stiff at normal temperatures but upon being raised to body temperature they soften and become very pliable and so adapt themselves very closely and comfortably to the body of the wearer.

The following example shows one method for the preparation of emulsions according to the invention without in any way limiting the same:

Start by mixing and heating in an aluminum vessel containing no copper or iron parts:

Grams Water 3000 Emulphur-O 420 Benzoyl peroxide 9 Benzyl alcohol 120 Normal propanol 720 After solution add:

Pure monomeric vinyl acetate 6000 Carefully maintain at boiling for 5 hours in a water bath, the vessel being provided with a reflux condenser and a thermometer.

At the end of this period the emulsion is cooled by circulating cold water in the bath while stirring the reaction mass.

It will be noted in the above example that vinyl acetate is present in greater amount than all of the other ingredients combined, roughly 58% of the total mix. The emulgent is used in the proportion of 7% of the vinyl acetate.

This yields a sort of cream containing an excess of monomeric vinyl acetate. This excess however is harmless for the proposed applications.

Now this emulsion, thickened for example with dextrines or kindred substances, may be applied by a scraper on reverse side of velvets. By this method a sufiiciently permanent sizing is produced. Such a sizing softens between 35 and The softening points of the emulsions may be raised by (a) increasing the time of polymerisation; (b) decreasing the amount of polymerisation catalyst; (c) decreasing the amount of plastifier.

In the above example the monomeric vinyl acetate is partly dissolved in the n-propanol which is, in turn, partly dissolved in the water. The plasticizer, benzyl alcohol, is soluble in both the water and the n-propanol. Emulphur-O assists in keeping the monomeric vinyl acetate in suspension and emulsifies the polymer as it is formed. The benzoyl peroxide is a. polymerisation catalyst. The polymerisation product remains right in the emulsion and at no time separates out.

The ingredientsabove set out are only by way of example. In place of benzoyl peroxide any of a large number of polymerisation catalysts may be used, the usual ones being oxidizing agents including other organic peroxides or ozonides, metallic oxides capable of yielding oxygen etc.

Benzyl alcohol may be replaced soluble plasticizers.

Normal propanol may be replaced by other low molecular weight alcohols as noted above.

The proportions existing among the ingredients may be varied within wide ranges to produce sizing compositions of different properties. The solvent content, water and n-propanol in the example, may be varied to change the viscosity of the product. The plasticizer may be varied to produce a size of more or less plasticity. The emulgent content may be varied to change the viscosity of the product.

Having now explained the invention and given an example thereof what is claimed is:

1. A process for the preparation of textile sizings comprising, mixing water, a low molecular weight water soluble alcohgl, a water soluble plasticizer, an emulgent comprising the lauric ether of polyethylene oxide, and a polymerisation catalyst; adding to said mix monomeric vinyl acetate; said emulgent being present as from 5 to 20% of the vinyl acetate; and heating the resulting mix to polymerise the vinyl acetate.

2. A process for the preparation of a textile sizing which comprises the steps of mixing water, lauric ether of polyethylene oxide, benzoyl peroxide, benzyl alcohol, and n-propanol; thereafter adding monomeric vinyl acetate; and refluxing the resulting mixture for a time sufllcient to polymerise a substantial part of the vinyl acetate.

3. The process of preparing a textile sizing which comprises the steps of mixing water 3000 g., lauric ether of polyethylene oxide 420 g., benzoyl peroxide 9 g., benzyl alcohol 120 g., n-propanol 720 g.; adding 6000 g. monomeric vinyl acetate;

by other water and refluxing the resulting mixture for about 5 hours.

4. A textile sizing comprising polymerised vinyl acetate, water, a water soluble alcohol of low boiling point, a water soluble plasticizer having a free alcoholic function, and an emulgent comprising the lauric ether of polyethylene oxide.

5. The process of preparing an emulsion comprising mixing minor portions of water, a water soluble alcohol, and the lauric ether of polyethylene oxide; adding thereto a major portion of monomeric vinyl acetate; and polymerising the vinyl acetate to form an emulsion directly.

6. An emulsion comprising polymerised vinyl acetate, water, a low molecular weight water soluble alcohol, and lauric ether of polyethylene oxide in the proportion of from 5 to 20% of the vinyl acetate.

SEARCH 300i 7. An emulsion comprising a major proportion of polymerised vinyl acetate, and minor proportions of water and a low molecular weight water soluble alcohol and lauric ether of polyethylene oxide.

8. An emulsion comprising water, a water soluble alcohol, a water soluble plasticizer, an emulgent comprising the lauric ether of polyethylene oxide, and polymerised vinyl acetate.

9. An emulsion of polymerised vinyl acetate in 10 polymerised vinyl acetate a major 15 

